CN109292737A - A kind of application method preparing hydrogen fluoride recirculating fluidized bed degasser - Google Patents
A kind of application method preparing hydrogen fluoride recirculating fluidized bed degasser Download PDFInfo
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- CN109292737A CN109292737A CN201811207311.XA CN201811207311A CN109292737A CN 109292737 A CN109292737 A CN 109292737A CN 201811207311 A CN201811207311 A CN 201811207311A CN 109292737 A CN109292737 A CN 109292737A
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- liquid
- hydrogen fluoride
- fluidized bed
- multistage cyclone
- recirculating fluidized
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
- C01B7/196—Separation; Purification by distillation
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The present invention relates to technical field of fluorine chemical industry, and in particular to a kind of application method for preparing hydrogen fluoride recirculating fluidized bed degasser, it is characterized in that: removing heavy constituent H after rectifying2SO4、H2Hydrogen fluoride liquid after O is taken over from feed liquid of the design in the middle part of recirculating fluidized bed degassing tower body to be entered, and liquid-bearing pan, its volatile components SO when hydrogen fluoride liquid flows to level-one grade finned surface plate under are injected2、SiF4、CO2、H2S to form upflowing vapor by gasifying, and is continuously improved through the tower bottom difficulty volatile component hydrogen fluoride liquid purity that is enriched to that multistage cyclone separation condenser condenses out, to realize the purpose of removing light component.
Description
Technical field
The present invention relates to technical field of fluorine chemical industry, and in particular to a kind of to prepare making for hydrogen fluoride recirculating fluidized bed degasser
Use method.
Background technique
Hydrogen fluoride is widely used to the industries such as electronics, chemical industry, petroleum, is mainly used as producing villiaumite, fluorohaloparaffin, fluorine cause
Cryogen, etching glass, impregnated timber, electrolysis element fluorine etc., degasser is to produce one of anhydrous hydrogen fluoride key equipment.In
(Patent No. CN 201720751304.0, patent name are a kind of degassing for anhydrous hydrogen fluoride production to state's patent of invention
Tower) disclose a kind of degassing tower for anhydrous hydrogen fluoride production, it is characterised in that including tower body, the tower body intracavity bottom
Two sides are respectively connected with support rod, interior tower are connected at the top of the support rod, the bottom of the interior tower is connected to discharge nozzle, described interior
Bottom on the right side of tower is connected to branch pipe, is connected with air blower on the right side of the branch pipe, the inner cavity of the interior tower is connected with filler, described
The top of diversion pipe and the bottom of distributive pipe connect, and are connected with supporting plate, the surface etc. of the supporting plate at the top of the tower body inner cavity
Distance offers venthole, and the bottom of the supporting plate is equidistant to be connected with water collecting piece, the top and bottom on the left of the water collecting piece
It is respectively connected with water blocking tooth, the bottom of the water collecting piece is connected with the tip that drips.The present invention has production when anhydrous hydrogen fluoride deaerates
Raw liquid will not flow to the advantage in air, and degassing can be reduced by solving liquid and flowing to cause damages to air in air
The problem of tower practicability.(Patent No. CN 201210506779.5, patent name are a kind of anhydrous fluorination to Chinese invention patent
The preparation method of hydrogen) disclose a kind of preparation method of anhydrous hydrogen fluoride, comprising the following steps: it a) will mixing sulfuric acid and fluorspar powder
After heating respectively, is mixed in pre-reactor according to certain feed weight ratio and carry out pre-reaction, obtain mixed material；It b) will mixing
Material is continuously fed into converter reactor, is performed under heating conditions reaction, obtains thick hydrogen fluoride gas and solid material, will
A part of obtained solid material is fed to converter reactor secondary response again by material-returning device, and remaining solid material enters two
Water gypsum process units；C) the washed tower of thick hydrogen fluoride gas, condenser, rectifying column and degassing tower processing, obtain pure fluorine
Change hydrogen and residual gas；D) circulation and stress is carried out to residual gas using sulfuric acid, to absorb hydrogen fluoride gas；E) it is not followed
The residual gas that loopback is received is discharged after water scrubber processing and tail gas tower processing from tail gas tower top.
The technical solution that the prior art 1 and the prior art 2 propose is degassing tower, current degassing tower be generally plate column or
It using the packed tower of structured packing, selects packed tower as degasification technique device, is suitable for quick and moment reaction process, has
The low advantage of high specific surface area, high gas film mass transfer coefficient, gas phase flow pressure drop, the disadvantage is that liquid storage amount is small, liquid is in filler
Tower residence time is shorter；It selects plate column as rectification process device, is suitable for quick and middling speed reaction process, there is liquid
The advantage that back-mixing is small, the residence time is uniform, film mass transfer coefficient is larger, the disadvantage is that structure is complicated, gas-phase pressure drop is big, tower internals not
It is corrosion-resistant.To sum up, due to the limitation of packed tower and plate column liquid storage amount, the ability of processing is small, and mass-transfer efficiency is low, and pressure drop is big,
Operating flexibility is small.
Summary of the invention
In view of the deficiencies of the prior art, hydrogen fluoride recirculating fluidized bed degasser is prepared the object of the present invention is to provide a kind of
Application method, it is characterized in that:
Step 1 uses the preceding liquid level shape that the U-shaped fluid-tight device in II bottom of multistage cyclone separation condenser must be observed by liquidometer
Condition guarantees that liquid level is higher than material returning device at least 300mm, it is ensured that U-shaped fluid-tight device is in normal operating conditions.
Step 2 removes heavy constituent H after rectifying2SO4、H2Hydrogen fluoride liquid after O is from design in recirculating fluidized bed degassing tower
Feed liquid in the middle part of body, which is taken over, to be entered, and is injected liquid-bearing pan, is injected 19.5 ± 0.5 DEG C of temperature, hydrogen fluoride liquid is uniformly distributed through liquid-bearing pan
After drip thermostat, thermostat includes permanent hot tubulation and finned surface plate, and oven heated temperature is 19.5 ± 0.5 DEG C, hydrogen fluoride liquid
Its volatile components SO when flowing to level-one grade finned surface plate under2、SiF4、CO2、H2S to form upflowing vapor by gasifying, across holding liquid
Disk enters multistage cyclone separation condenser I, and it is 9~19 DEG C cold that the design of multistage cyclone separation condenser I, which has collet and is passed through temperature,
But water, the drop that upflowing vapor carries form continuous liquid film on I stack shell wall of multistage cyclone separation condenser through cyclonic separation, on
Enter the external multistage cyclone separation condenser II of recirculating fluidized bed degassing tower after rising steam and the abundant mass transfer of dirty liquid film, it is multistage
It is 9~19 DEG C of cooling waters that cyclonic separation condenser II, which is similarly designed with collet and is passed through temperature, and upflowing vapor is volatile at this time
Component SO2、SiF4、CO2、H2S content is continuously improved, the difficult volatile component fluorine condensed out through multistage cyclone separation condenser II
Change hydrogen liquid purity to be continuously improved, the design of II bottom of multistage cyclone separation condenser has U-shaped fluid-tight device and material returning device, and hydrogen fluoride liquid returns
Returning liquid-bearing pan becomes phegma, the phegma that multistage cyclone separation condenser I condenses out in recirculating fluidized bed degassing tower body
Again through liquid-bearing pan downstream to thermostat, then the difficult volatile component hydrogen fluoride liquid hold-up of tower bottom enrichment is higher and higher, thus real
Light component SO is showed2、SiF4、CO2、H2The removing of S.
Inventors have found that preparing the fluorite (CaF of hydrogen fluoride2) and sulfuric acid (H2SO4) following main reaction: CaF occurs2+
2H2S04→2HF+CaSO4, the product into the subsequent processing stage mainly has heavy constituent H2SO4、H2O, light component SO2、SiF4、
CO2、H2S, byproduct include CaSO4、Fe2(SO4)3、H2SiF6.It is marked according to " anhydrous hydrogen fluoride for industrial use " GB 7746-2011 country
Quasi- requirement, to H2SO4、H2O、H2SiF6、SO2Content it is restricted, prepare anhydrous hydrogen fluoride be usually utilize above-mentioned each group
Divide the difference of boiling point to realize the removal of impurity using the process of washing, condensation, rectifying, degassing, is specifically exactly hydrogen fluorine
Acid gas enters scrubbing tower from reacting furnace and is washed, and after removing dust, water impurity, enters condenser system by scrubbing tower, passes through
Level-one, second level, three-level condensation, level-one condense to be formed thick liquid HF acid (main component be heavy constituent H2SO4、H2O washing) is returned
Tower condensation washing hydrofluoric acid gas, the thick liquid HF acid (main component is hydrofluoric acid) that second level, three-level condense out is by rectifying
It is pumped into degassing tower, further removes light component SO in rectifying column2、SiF4、CO2、H2S and heavy constituent H2SO4、H2O is obtained anhydrous
Hydrogen fluoride finished product.
Inventors have found that hydrogen fluoride finished product preparation process selection be usually rectifying and degasification technique, i.e., using hydrogen fluoride with
The volatilization gender gap of other components, takes multiple equilibrium process, multi-component mixture is isolated pure hydrogen fluoride.No matter adopt
It is all using phegma and upper with being that first light (component) weighs (component) afterwards or first weigh the process flow of (component) light (component) afterwards
Gas is risen, forms gas-liquid counter current contact in a distillation column, the difficult volatile component in uprising gas constantly condenses, while its not disconnecting again
The volatile components for gasifying out in the phegma flowed from the top down are received, therefore on it during liter, wherein volatile components
Content be continuously improved, from the higher volatile components product of the available purity in the top of tower, another aspect phegma is at it
In downflow processes, volatile components therein constantly gasify, while it constantly receives the difficulty condensed out in upflowing vapor again and waves
Component is sent out, so wherein the content of difficult volatile component is continuously improved, the higher difficult volatilization group of available purity in the bottom of tower
Divide product.
Inventors have found that the energy handled in prior art plate column or packed tower can be overcome using recirculating fluidized bed degassing
Power is small, and mass-transfer efficiency is low, and pressure drop is big, the small disadvantage of operating flexibility.Recirculating fluidized bed degassing tower body is divided into two sections, and top is
Rectifying section, lower part are stripping section, and rectifying section design has multistage cyclone separation condenser I, multistage cyclone separation condenser II, stripping
Section design has thermostat, and heavy constituent H is removed after rectifying2SO4、H2Hydrogen fluoride liquid after O is from design in recirculating fluidized bed degassing tower
Feed liquid in the middle part of body, which is taken over, to be entered, and is injected liquid-bearing pan, is injected 19.5 ± 0.5 DEG C of temperature, hydrogen fluoride liquid is uniformly distributed through liquid-bearing pan
After drip thermostat, thermostat includes permanent hot tubulation and finned surface plate, and oven heated temperature is 19.5 ± 0.5 DEG C, hydrogen fluoride liquid
Its volatile components SO when flowing to level-one grade finned surface plate under2、SiF4、CO2、H2S to form upflowing vapor by gasifying, across holding liquid
Disk enters multistage cyclone separation condenser I, and it is 9~19 DEG C cold that the design of multistage cyclone separation condenser I, which has collet and is passed through temperature,
But water, the drop that upflowing vapor carries form continuous liquid film on I stack shell wall of multistage cyclone separation condenser through cyclonic separation, on
Enter the external multistage cyclone separation condenser II of recirculating fluidized bed degassing tower after rising steam and the abundant mass transfer of dirty liquid film, it is multistage
It is 9~19 DEG C of cooling waters that cyclonic separation condenser II, which is similarly designed with collet and is passed through temperature, and upflowing vapor is volatile at this time
Component SO2、SiF4、CO2、H2S content is continuously improved, the difficult volatile component fluorine condensed out through multistage cyclone separation condenser II
Change hydrogen liquid purity to be continuously improved, the design of II bottom of multistage cyclone separation condenser has U-shaped fluid-tight device and material returning device, and hydrogen fluoride liquid returns
Returning liquid-bearing pan becomes phegma, the phegma that multistage cyclone separation condenser I condenses out in recirculating fluidized bed degassing tower body
Again through liquid-bearing pan downstream to thermostat, then the difficult volatile component hydrogen fluoride liquid hold-up of tower bottom enrichment is higher and higher, thus real
Light component SO is showed2、SiF4、CO2、H2The removing of S.
Inventors have found that the purpose of setting multistage cyclone separation condenser I is treated as increasing in recirculating fluidized bed degassing tower body
Interconderser, makes operation lines closer to balanced line, reduces the invertibity of degasification process, improve thermodynamic efficiency.
Inventors have found that the structure relative to plate column column plate complexity, multistage cyclone separation condenser have structure it is simple,
Cheap advantage, while cyclone liquid gas separation, stack shell inner wall liquid film easy to form, upflowing vapor are sufficiently passed with dirty liquid film
The characteristics of matter, makes it have the advantage that plate column liquid dispersion is small, film mass transfer coefficient is larger, while multi-cyclone has
Standby multiple equilibrium stages or theoretical tray, can be arranged, and the pressure drop of cyclone separator is lower according to actual needs, compare filler
Tower has more power savings advantages.
Compared with the existing technology, the present invention, which at least contains, has the advantage that first, the knot relative to plate column column plate complexity
Structure, multistage cyclone separation condenser have the advantages that structure is simple, cheap, while cyclone liquid gas separation, stack shell inner wall are held
The characteristics of easily forming liquid film, upflowing vapor and dirty liquid film abundant mass transfer makes it have that plate column liquid dispersion is small, film mass transfer
The larger advantage of coefficient, while multi-cyclone has multiple equilibrium stages or theoretical tray, can give according to actual needs
Setting, and the pressure drop of cyclone separator is lower, has more power savings advantages than packed tower；Second, in recirculating fluidized bed degassing tower body
The purpose that multistage cyclone separation condenser I is arranged is treated as increasing interconderser, makes operation lines closer to balanced line, reduces
The invertibity of distillation process, improves thermodynamic efficiency.
Detailed description of the invention
Fig. 1 is a kind of front view structure signal of application method for preparing hydrogen fluoride recirculating fluidized bed degasser of the present invention
Figure.
Fig. 2 is a kind of plan structure signal of application method for preparing hydrogen fluoride recirculating fluidized bed degasser of the present invention
Figure.
Fig. 3 is a kind of A partial enlargement structure for the application method for preparing hydrogen fluoride recirculating fluidized bed degasser of the present invention
Schematic diagram.
I 2- recirculating fluidized bed of 1- multistage cyclone separation condenser degassing tower body 3- feed liquid adapter tube
The permanent hot tubulation 6- finned surface plate 7- multistage cyclone separation condenser II of 4- thermostat 5-
8-U type fluid-tight device 9- material returning device 10- liquid-bearing pan.
Specific embodiment
The present invention is described further with specific embodiment with reference to the accompanying drawing.
As shown in Figure 1, Figure 2, Figure 3 shows, a kind of application method preparing hydrogen fluoride recirculating fluidized bed degasser, feature
It is:
Step 1 uses the preceding liquid level that the U-shaped fluid-tight device 8 in II 7 bottom of multistage cyclone separation condenser must be observed by liquidometer
Situation guarantees that liquid level is higher than at least 300mm of material returning device 9, it is ensured that U-shaped fluid-tight device 8 is in normal operating conditions.
Step 2 removes heavy constituent H after rectifying2SO4、H2Hydrogen fluoride liquid after O is from design in recirculating fluidized bed degassing tower
The feed liquid adapter tube 3 at 2 middle part of body enters, and injects liquid-bearing pan 10, injects 19.5 ± 0.5 DEG C of temperature, hydrogen fluoride liquid is equal through liquid-bearing pan 10
Thermostat 4 is dripped after even distribution, thermostat 4 includes permanent hot tubulation 5 and finned surface plate 6, and 4 heating temperature of thermostat is 19.5 ± 0.5
DEG C, its volatile components SO when hydrogen fluoride liquid flows to level-one grade finned surface plate 6 under2、SiF4、CO2、H2S, which is formed to rise by gasification, to be steamed
Vapour passes through liquid-bearing pan 10 and enters multistage cyclone separation condenser I 1, and the design of multistage cyclone separation condenser I 1 has collet and is passed through
Temperature is 9~19 DEG C of cooling waters, and the drop that upflowing vapor carries is through cyclonic separation in I 1 stack shell wall of multistage cyclone separation condenser
Upper to form continuous liquid film, the multistage entered outside recirculating fluidized bed degassing tower body 2 after upflowing vapor and the abundant mass transfer of dirty liquid film is revolved
Wind separation condenser II 7, it is 9~19 DEG C of cooling waters that multistage cyclone separation condenser II 7, which is similarly designed with collet and is passed through temperature,
The volatile components SO of upflowing vapor at this time2、SiF4、CO2、H2S content is continuously improved, cold through multistage cyclone separation condenser II 7
It coagulates the difficult volatile component hydrogen fluoride liquid purity got off to be continuously improved, the design of II 7 bottom of multistage cyclone separation condenser has U-shaped fluid-tight
Device 8 and material returning device 9, hydrogen fluoride liquid, which returns to liquid-bearing pan 10, becomes phegma, multistage cyclone separation in recirculating fluidized bed degassing tower body 2
The phegma that condenser I 1 condenses out is also again through liquid-bearing pan 10 downstream to thermostat 4, then the difficult volatilization group of tower bottom enrichment
Divide hydrogen fluoride liquid hold-up higher and higher, to realize light component SO2、SiF4、CO2、H2The removing of S.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to of the invention
Some modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although being used in this specification
Some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (1)
1. a kind of application method for preparing hydrogen fluoride recirculating fluidized bed degasser, it is characterized in that: step 1, must lead to before
The liquid level situation for crossing the liquidometer observation U-shaped fluid-tight device in II bottom of multistage cyclone separation condenser guarantees that liquid level is higher than material returning device extremely
Few 300mm, it is ensured that U-shaped fluid-tight device is in normal operating conditions；Step 2 removes heavy constituent H after rectifying2SO4、H2Fluorine after O
Change hydrogen liquid is taken over from feed liquid of the design in the middle part of recirculating fluidized bed degassing tower body to be entered, injection liquid-bearing pan, and injection temperature 19.5 ±
0.5 DEG C, hydrogen fluoride liquid drips thermostat after liquid-bearing pan is uniformly distributed, and thermostat includes permanent hot tubulation and finned surface plate, thermostat
Heating temperature is 19.5 ± 0.5 DEG C, its volatile components SO when hydrogen fluoride liquid flows to level-one grade finned surface plate under2、SiF4、CO2、
H2S to form upflowing vapor by gasifying, and enters multistage cyclone separation condenser I across liquid-bearing pan, multistage cyclone separation condenser I is set
In respect of collet and temperature is passed through as 9~19 DEG C of cooling waters, and the drop that upflowing vapor carries is separated through cyclonic separation in multistage cyclone
Continuous liquid film is formed on I stack shell wall of condenser, enters recirculating fluidized bed degassing tower after upflowing vapor and the abundant mass transfer of dirty liquid film
External multistage cyclone separation condenser II, multistage cyclone separation condenser II be similarly designed with collet and be passed through temperature be 9~
19 DEG C of cooling waters, at this time the volatile components SO of upflowing vapor2、SiF4、CO2、H2S content is continuously improved, and separates through multistage cyclone
The difficult volatile component hydrogen fluoride liquid purity that condenser II condenses out is continuously improved, the design of II bottom of multistage cyclone separation condenser
There are U-shaped fluid-tight device and material returning device, hydrogen fluoride liquid, which returns to liquid-bearing pan, becomes phegma, multistage cyclone in recirculating fluidized bed degassing tower body
The phegma that separation condenser I condenses out is also again through liquid-bearing pan downstream to thermostat, then the difficult volatilization group of tower bottom enrichment
Divide hydrogen fluoride liquid hold-up higher and higher, to realize light component SO2、SiF4、CO2、H2The removing of S.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811207311.XA CN109292737B (en) | 2018-10-17 | 2018-10-17 | Use method of circulating fluidized bed degassing device for preparing hydrogen fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811207311.XA CN109292737B (en) | 2018-10-17 | 2018-10-17 | Use method of circulating fluidized bed degassing device for preparing hydrogen fluoride |
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| CN109292737A true CN109292737A (en) | 2019-02-01 |
| CN109292737B CN109292737B (en) | 2020-03-10 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1174382A (en) * | 1967-12-14 | 1969-12-17 | Maxim Ivanovich Kafyrov | A Method for Purifying Hydrofluoric Acid. |
| JPS57106503A (en) * | 1980-12-22 | 1982-07-02 | Mitsubishi Gas Chem Co Inc | Separation of hydrogen fluoride |
| CN201971632U (en) * | 2011-04-07 | 2011-09-14 | 多氟多化工股份有限公司 | Anhydrous hydrogen fluoride rectifying tower |
| CN103818880A (en) * | 2014-03-05 | 2014-05-28 | 宣城亨泰化工科技有限公司 | Production system for electronic-grade hydrofluoric acid |
| CN207016471U (en) * | 2017-06-27 | 2018-02-16 | 江西天晟化工有限公司 | A kind of degassing tower for anhydrous hydrogen fluoride production |
| CN108313983A (en) * | 2018-05-03 | 2018-07-24 | 繁昌县凯艺电子商务有限公司 | The hydrofluoric acid purifying prepared for high purity lithium fluoride and preparation method |
-
2018
- 2018-10-17 CN CN201811207311.XA patent/CN109292737B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1174382A (en) * | 1967-12-14 | 1969-12-17 | Maxim Ivanovich Kafyrov | A Method for Purifying Hydrofluoric Acid. |
| JPS57106503A (en) * | 1980-12-22 | 1982-07-02 | Mitsubishi Gas Chem Co Inc | Separation of hydrogen fluoride |
| CN201971632U (en) * | 2011-04-07 | 2011-09-14 | 多氟多化工股份有限公司 | Anhydrous hydrogen fluoride rectifying tower |
| CN103818880A (en) * | 2014-03-05 | 2014-05-28 | 宣城亨泰化工科技有限公司 | Production system for electronic-grade hydrofluoric acid |
| CN207016471U (en) * | 2017-06-27 | 2018-02-16 | 江西天晟化工有限公司 | A kind of degassing tower for anhydrous hydrogen fluoride production |
| CN108313983A (en) * | 2018-05-03 | 2018-07-24 | 繁昌县凯艺电子商务有限公司 | The hydrofluoric acid purifying prepared for high purity lithium fluoride and preparation method |
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Effective date of registration: 20221110 Address after: No. 19, Gangcheng Road, Dongying Port Economic Development Zone, Dongying City, Shandong Province 257237 Patentee after: Dongying Ruigang Pipeline Engineering Co.,Ltd. Address before: 362000 the 2 floor of 32 new gate Street and 1916 Creative Industrial Park, Licheng District, Quanzhou, Fujian, China, 1916 Patentee before: Yang Song |
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